CN106883630A - A kind of calcium sulfate whisker modified pitch and preparation method thereof - Google Patents
A kind of calcium sulfate whisker modified pitch and preparation method thereof Download PDFInfo
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- CN106883630A CN106883630A CN201710279004.1A CN201710279004A CN106883630A CN 106883630 A CN106883630 A CN 106883630A CN 201710279004 A CN201710279004 A CN 201710279004A CN 106883630 A CN106883630 A CN 106883630A
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- calcium sulfate
- pitch
- whisker
- crystal whiskers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/08—Oxygen-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Road Paving Structures (AREA)
Abstract
The invention belongs to asphalt preparation field, disclose a kind of calcium sulfate whisker modified pitch and preparation method thereof, matrix pitch is heated to flow regime, flow regime is reheated to after sieving, then temperature constant state is kept to be stirred, the calcium sulfate crystal whiskers calcium sulfate crystal whiskers that mass percent is 2~8wt% are added while stirring, addition continues to stir and can obtain modified pitch after finishing.The present invention enters matrix pitch by being added using nearly nanoscale calcium sulfate crystal whiskers, change over the excessive phenomenon in many calcium sulfate whiskers fibre sections, its whisker section is set to reach nearly nano-scale, so as to make it have the characteristic that can be more fully contacted with pitch each component, preferably change pitch colloform texture, make that its pavement performance is more excellent, economy, and nearly nanoscale calcium sulfate crystal whiskers are in process of production, energy consumption is low, and itself is nontoxic, nonirritant, is this strategic industry policy for complying fully with national sustainable development.
Description
Technical field
The present invention relates to asphalt preparation field, a kind of calcium sulfate whisker modified pitch and its preparation side are specifically referred to
Method.
Background technology
Asphalt is typical viscoelastoplastic material, is softened when temperature is raised, and easily rut occurs under load action；
Temperature reduction time-varying cirrhosis is crisp, easily fatigue cracking and cold cracking occurs under load and temperature collective effect.
Modern rubber cement theory thinks that asphalt is a kind of Multistage dispersion system, although ratio is relatively small, but its
It is mostly important in dispersion, it is the influence viscoelastic basic factor of asphalt, the rheological behavior of asphalt mastic is to pitch
The permanent deformation resistance of compound has decisive influence, largely affects the performance of compound.According to the U.S.
" SHRP (SHRP) " achievement in research, asphalt mastic is 29% for the contribution rate of high temperature rut, to fatigue
Contribution rate is 52%, and the contribution rate to thermal cracking is 87%.Therefore pitch is most important wherein, so researcher is more next
More trials carry out modified pitch using fiber, inorganic filler, macromolecular material etc., but these materials are often difficult to while simultaneous
Modified effect and economy are turned round and look at, such as asbestos fibre is poisonous, consumed energy in basalt fibre production process very big, both environmental protection pressures
Power is big, and lignin fibre can cause the consumption of pitch to increase, and cost performance is low from the angle of economy.
The content of the invention
It is an object of the invention to：Overcome the deficiencies in the prior art, there is provided a kind of calcium sulfate whisker modified pitch and its system
Preparation Method.The present invention enters matrix pitch by being added using nearly nanoscale calcium sulfate crystal whiskers, and many calcium sulfate of changing over are brilliant
The excessive phenomenon in palpus product fibre section, makes its whisker section reach nearly nano-scale, so as to make it have and pitch each group
The characteristic that point can be more fully contacted, preferably changes pitch colloform texture, makes that its pavement performance is more excellent, economy, and
In process of production, energy consumption is low, and itself is nontoxic, nonirritant, is to comply fully with country to hold for nearly nanoscale calcium sulfate crystal whiskers
This strategic industry policy of supervention exhibition.
The present invention is achieved through the following technical solutions：
A kind of calcium sulfate whisker modified asphalt production process, flow regime is heated to by matrix pitch, is added again after sieving
Then heat keep temperature constant state to be stirred to flow regime, and the sulphur that mass percent is 2~8wt% is added while stirring
Sour calcium pyroborate calcium sulfate crystal whiskers, addition continues to stir and can obtain modified pitch after finishing.
As a preferred mode, selection is brilliant Sichuan Wan Run nonmetallic mineral materials Co., Ltd dead plaster
Palpus.
As a preferred mode, the mass percent of calcium sulfate crystal whiskers addition is 2wt%.
The mass percent of calcium sulfate crystal whiskers addition is 8wt% as a preferred mode.
The mass percent of calcium sulfate crystal whiskers addition is 4~6wt% as a preferred mode.
The mass percent of calcium sulfate crystal whiskers addition is 4wt% as a preferred mode.
The mass percent of calcium sulfate crystal whiskers addition is 6wt% as a preferred mode.
A kind of calcium sulfate whisker modified pitch, is obtained using the above method.
The present invention compared with prior art, with advantages below and beneficial effect：The present invention is by using nearly nanoscale sulphur
The addition of sour calcium pyroborate enters matrix pitch, changes over the excessive phenomenon in many calcium sulfate whiskers fibre sections, makes its crystalline substance
Palpus section reaches nearly nano-scale, so as to make it have the characteristic that can be more fully contacted with pitch each component, preferably changes
Pitch colloform texture, makes that its pavement performance is more excellent, economy, and nearly nanoscale calcium sulfate crystal whiskers are in process of production,
Energy consumption is low, and itself is nontoxic, nonirritant, is this strategic industry policy for complying fully with national sustainable development.
Brief description of the drawings
Fig. 1 is the temperature sensitive property coefficient influence figure of CSW volumes.
Fig. 2 is that CSW volumes influence to scheme on penetration index.
Fig. 3 is CSW addition contents to modified pitch viscosity influence figure.
Fig. 4 is CSW addition contents to the glutinous temperature exponential effect figure of modified pitch..
Specific embodiment
Further described in detail below in conjunction with the accompanying drawings, but embodiments of the present invention not limited to this：
Embodiment 1：
First, material and instrument
What calcium sulfate crystal whiskers were selected is Sichuan Wan Run nonmetallic mineral materials Co., Ltd anhydrous calcium sulfate whisker, main skill
Art index is shown in Table 1.So that conventional hydrothermal method prepares calcium sulfate crystal whiskers as an example, prepared by conventional anhydrous calcium sulfate whisker is that gypsum exists
The recrystallization common calcium sulfate crystal whiskers of generation are stirred in reactor, certain temperature and pressure are maintained in reactor.Its detailed process
Can be that the dihydrate gypsum suspension less than 2% is added in water autoclave to process, in saturated vapor pressure, dihydrate gypsum becomes
Into the semi-hydrated gypsum of tiny needle-like, then hemihydrate calcium sulfate crystal whisker is obtained through order treatment.Compared with conventional hydrothermal method, Sichuan ten thousand
The anhydrous calcium sulfate whisker that profit nonmetallic mineral material Co., Ltd is produced, preparation process difference is to add in a kettle.
There is nano molecular derivant, the nano molecular derivant is mot nano induction agent, is induced by the composition, nano molecular induction
Agent combination calcium sulfate molecule generates nearly nanoscale calcium sulfate crystal whiskers referred to herein.
Pitch uses Period In Maoming petrochemical industry East Sea AH70#, AH90#A grade of bi tumenf orr oad of board, and the key technical indexes is shown in Table
2。
Asphalt performance tests used pertinent instruments to be included：(the auspicious instrument in Shanghai side has SNB-1A-J types Brookfield viscometer
Limit company), JJ-1 types mechanical agitator (Taizhou Ai Ce Instrument Ltd.), YLRH-1 type asphalt softening point instrument (Xi'an AsiaSat
Building Instrument Ltd.), YX-1 type bitumen ductilities instrument (Xi'an AsiaSat building Instrument Ltd.), YLZ-1 type computer pins enter
Degree instrument (Xi'an AsiaSat building Instrument Ltd.).
The technical indicator of the ACS-01 anhydrous calcium sulfate whiskers of table 1
The technical indicator of East Sea board AH70# and the AH90# pitch of table 2
2nd, the preparation of calcium sulfate whisker modified pitch
Matrix pitch is heated to flow regime in 135 DEG C of baking ovens, 0.6mm standard screens are crossed, 500g is weighed while hot and is moved to
Continue to heat on electrothermal furnace equipped with temp controlled meter, after after temperature stabilization, stirred using mechanical agitator, be slowly added into quality percentage
Than the calcium sulfate crystal whiskers for being respectively 2~8wt%, continue to stir 30mi n, obtain modified pitch.
3rd, calcium sulfate whisker modified asphalt performance analysis
Calcium sulfate whisker modified pitch is pressed《Highway engineering pitch and Asphalt Mixture Experiment code》Carry out three norms
Test and determine that penetration index makees PI, using PI as the index for evaluating pitch response to temperature, test 15 DEG C, 30 DEG C of needle penetrations, press
Formula (1) seeks calculation penetration index：
A values are temperature sensitivity coefficient A in formula (1), and its computational methods is using between penetration values and temperature
Linear relationship, regression straight line is sought by three temperature and corresponding needle penetration, and its slope is temperature sensitivity coefficient A, can
Asked for by least square method, Chang An University's thesis for the doctorate that least square method is made for prosperous 2006 referring to Chen Hua《SBS modified pitch
Pavement performance and study mechanism》.Formula (2) is：
3rd, brookfield viscosity experiment
The modified pitch that 2wt%, 4wt%, 6wt%, 8wt% are respectively to matrix pitch and content of modifier carries out Bu Shi
Viscosity test, test temperature is respectively 135 DEG C and 175 DEG C, and viscous temperature is sought according to the algorithmic formula (3) that temperature index is sticked under Celsius' thermometric scale
Index, and further influence of the analysis calcium sulfate crystal whiskers and its addition content to viscosity.Algorithmic formula (3) is：
4th, the key property of modified pitch
Influence result of the test of the different calcium sulfate crystal whiskers mix ratios to pitch three norms is as shown in table 3.
The modified asphalt technology index of table 3
From the result of table 3, as calcium sulfate crystal whiskers addition content increases to 8wt% from 0wt%, 70# asphalt softening points from
47.45 DEG C of matrix pitch increase to 53..85 DEG C, and the softening point of 90# pitches is increased to from 46.70 DEG C of matrix pitch
51..65 DEG C, it is proportionate between softening point and whisker addition content.And with whisker addition content increase, 70# Asphalt Penetrations from
76.9 (0.1mm) are down to 35.3 (0.1mm) 90# Asphalt Penetrations and are down to 50.2 (0.1mm) from 86.4 (0.1mm), needle penetration and
It is negatively correlated between whisker addition content.
This be due in the presence of mechanical agitation, calcium sulfate crystal whiskers with slight fiber shape form it is unordered be dispersed in matrix
In pitch, because its intensity is high, good toughness, certain space lattice is formd in pitch matrix, hinder the flowing of pitch
Property, viscosity increases, therefore softening point increases, and needle penetration declines.With the increase of whisker addition content at 25 DEG C, modified pitch ductility
On a declining curve, ductility is reduced to below 100cm when 70# pitch whiskers volume is more than wt4%, illustrates with whisker addition content
Increase ductility decline, the plasticity reduction of pitch.This be because calcium sulfate crystal whiskers belong to rigid filled, it is rigid filled in composite wood
Its plastic deformation ability is quickly reduced with the increase of rigid particles in material, when tensile stress acts on modified pitch, matrix
Asphalt modulus are lower than calcium sulfate crystal whiskers modulus, and larger deformation is produced in the stretching direction, and whisker is passed with the stress of basal body interface
The ability of passing is destroyed, and causes asphalt test piece to be broken in advance, is macroscopically being presented as that elongation at break significantly reduces, and is limited
The plastic deformation ability of pitch, therefore ductility decline.And 90# pitches are larger due to mobility itself, so ductility reduction is less
Substantially.In summary analyze, whisker addition content is unsuitable excessive, it may be considered that mixing the calcium sulfate crystal whiskers with 4wt% -6wt% improves
Pitch key property.
5th, influence of the calcium sulfate crystal whiskers to penetration index
By parallel laboratory test respectively to matrix pitch and calcium sulfate crystal whiskers addition content 2wt%, 4wt%, 6wt%, 8wt%
Modified pitch test 30 DEG C, 25 DEG C, 15 DEG C of penetration number, calculated respectively by formula (1) and (2) temperature sensitivity coefficient A with
And penetration index PI.Experiment test and result of calculation are as shown in table 4, further to the temperature sensitivity of different whisker addition contents
Coefficient A maps with penetration index PI results, as depicted in figs. 1 and 2.Fig. 1 is the temperature sensitive property coefficient influence of CSW volumes
Figure.Fig. 2 is that CSW volumes influence to scheme on penetration index.
The modified pitch penetration number of table 4 and relevant temperature sensitivity coefficient A and penetration index PI
From the result of table 4 and Fig. 1, Fig. 2, as whisker addition content increases to 8wt%, 70# asphalt temperature sensitiveness from 0
Coefficient is reduced to 0.0233 from the 0.0270 of matrix pitch, and penetration index increases to 4.1514 from 2.7524, and 90# pitch temperature
Degree sensitivity coefficient is reduced to 0.0204 from the 0.0246 of matrix pitch, and penetration index increases to 4.8263, two from 3.4610
The temperature sensitivity coefficient for planting pitch is negatively correlated with calcium sulfate crystal whiskers addition content, and penetration index is filled with calcium sulfate crystal whiskers
Amount is proportionate.Should test result indicate that asphalt material add calcium sulfate crystal whiskers after, temperature sensitivity reduction, so as to increased
The high-temperature stability of asphalt material, the result matches with softening point test result.This be due to being acted in high-speed stirred under, sulphur
Sour calcium pyroborate is dispersed in pitch, and pitch to can be regarded as the dispersed phase that the different component of polarity constituted dispersed
In (slightly) decentralized medium containing polarity such as fragrance point, saturation are not divided, the light component in matrix pitch, such as oily wax, saturation point, virtue
Perfume (or spice) grades by permeating, diffusing into calcium sulfate crystal whiskers, causes the distance between pitch micelle and micelle to reduce, between micelle
Attraction increases, and these changes all make the reduction of asphalt temperature sensitiveness.
6th, influence of the calcium sulfate crystal whiskers to viscosity and viscosity-temperature index
The modified pitch that matrix pitch and whisker addition content are respectively 2wt%, 4wt%, 6wt%, 8wt% is existed respectively
Brookfield viscosity experiment is carried out under the conditions of 135 DEG C and 175 DEG C, the influence of analysis modifying agent and addition content to viscosity, experimental result is shown in
Table 5, the further viscosity to different whisker addition contents and the mapping of viscosity-temperature index result, as shown in Figure 3 and Figure 4.Fig. 3 mixes for CSW
Dosage is to modified pitch viscosity influence figure.Fig. 4 is CSW addition contents to the glutinous temperature exponential effect figure of modified pitch.
The Bu Luoke Fields viscosity and viscosity-temperature index of the modified pitch of table 5
As can be seen from Table 5, under conditions of calcium sulfate crystal whiskers are constant, with the increase of temperature, asphalt viscosity reduction, this master
If because with the increase pitch of temperature from elasticity to viscosity transformation [15], showing as viscosity decline.Can by table 5 and Fig. 3 results
Know, at the same temperature, two kinds of matrix pitches show as increasing with the addition content of calcium sulfate crystal whiskers, the brookfield viscosity of pitch
Gradually increase.By four component analysis of pitch, increasing asphalitine or reduce colloid can directly improve the colloform texture of pitch
[16-17].With the increase of calcium sulfate crystal whiskers addition content, free pitch is largely combined with whisker, in whole system, is freely dripped
Blue or green content is relative to be reduced, asphalitine ratio relative increase, and pitch becomes sticky, and whisker plays strengthening action, in pitch
The increase of abundance causes in the presence of external force in rubber cement, frictional resistance increase between whisker-whisker, therefore viscosity increases.
Viscosity-temperature index VTS reflects the viscosity-temperature characteristic of pitch, if the viscosity of pitch varies with temperature rate small, viscosity-temperature characteristic
It is good.From the point of view of measuring and calculation result, from table 5 and Fig. 4：Admixture whisker amount increases to 8wt%, 70# pitches VTS from 0wt%
Absolute value brings up to 3.437 from the 3.283 of matrix pitch, and 90# pitch VTS absolute values bring up to from the 3.063 of matrix pitch
3.981, unmodified pitch is above, and VTS absolute values increase as whisker addition content increases.This shows modified pitch
Temperature stability is improved, and with the increase of calcium sulfate crystal whiskers addition content, improvement amplitude has been lifted.Its reason is main
Be anhydrous calcium sulfate whisker heat-resisting quantity it is good, specific surface area is big, belongs to trickle monocrystal material, it is believed that be a kind of micro-
Fiber type, because with the increase of Whisker Content, the number of grid formed between whisker increases [18-19], so as to reduce pitch
Rheological characteristic, and the acidic resins in pitch have very strong surface-active, it can be such that whisker closely combines with pitch, this
The cementation for planting pitch of the combination specific ionization outside whisker is many by force, modified pitch is had more preferable heat resistance [20],
So addition calcium sulfate crystal whiskers increase asphalt high-temperature non-deformability, temperature stability improves.
Conclusion：
(1) three norms test is carried out to the pitch for filling calcium sulfate crystal whiskers, with the increase of whisker addition content, needle penetration
Reduce, softening point is raised, ductility reduction.Comprehensive various aspects of performance considers whisker mix ratio for 4~6wt% can preferably improve drip
Blue or green key property.
(2) influence of the analysis calcium sulfate crystal whiskers addition content to asphalt temperature sensitiveness, in 0~8wt% of whisker addition content
Scope, the modified pitch of two kinds of matrix pitch formation shows as increasing with the increase asphalt penetration index of mix ratio,
Temperature sensitivity reduction.
(3) in calcium sulfate crystal whiskers addition content 0~8wt% scopes, the volume with whisker increases, and asphalt viscosity increase is glued
Warm index | VTS | increases, the modified temperature stability that can effectively improve pitch of admixture of calcium sulfate crystal whiskers.
To sum up, it may be considered that used in sunshine-duration summer it is long, temperature is higher, the regional road that is required to high temperature Rut resistance
With 4~6wt% calcium sulfate crystal whiskers can be added to improve its high-temperature stability in pitch.
The above, is only presently preferred embodiments of the present invention, not does any formal limitation to the present invention, it is every according to
Any simple modification, the equivalent variations made to above example according to technical spirit of the invention, each fall within protection of the invention
Scope.
Claims (8)
1. a kind of calcium sulfate whisker modified asphalt production process, it is characterised in that：Matrix pitch is heated to flow regime, is sieved
After be reheated to flow regime, then keep temperature constant state be stirred, while stirring add mass percent be 2~
The nearly nanoscale calcium sulfate crystal whiskers of 8wt%, addition continues to stir and can obtain modified pitch after finishing.
2. a kind of calcium sulfate whisker modified asphalt production process according to claim 1, it is characterised in that：What is selected is four
The profit nonmetallic mineral material Co., Ltd of river ten thousand anhydrous calcium sulfate whisker.
3. a kind of calcium sulfate whisker modified asphalt production process according to claim 1 and 2, it is characterised in that：Calcium sulfate
The mass percent of whisker addition is 2wt%.
4. a kind of calcium sulfate whisker modified asphalt production process according to claim 1 and 2, it is characterised in that：Calcium sulfate
The mass percent of whisker addition is 8wt%.
5. a kind of calcium sulfate whisker modified asphalt production process according to claim 1 and 2, it is characterised in that：Calcium sulfate
The mass percent of whisker addition is 4~6wt%.
6. a kind of calcium sulfate whisker modified asphalt production process according to claim 5, it is characterised in that：Calcium sulfate crystal whiskers
The mass percent of addition is 4wt%.
7. a kind of calcium sulfate whisker modified asphalt production process according to claim 6, it is characterised in that：Calcium sulfate crystal whiskers
The mass percent of addition is 6wt%.
8. a kind of calcium sulfate whisker modified pitch, it is characterised in that：It is obtained using any one of claim 1~7.
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Cited By (2)
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| CN115960470A (en) * | 2022-12-30 | 2023-04-14 | 江苏中亿通道路新材料有限公司 | Fiber hydrophobic high-viscosity modified asphalt and preparation method thereof |
| CN116004020A (en) * | 2022-12-16 | 2023-04-25 | 广州市北二环交通科技有限公司 | Preparation method of self-healing pre-curing asphalt |
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Application publication date: 20170623 |